Residual solvent recovery apparatuses and methods

ABSTRACT

The disclosed embodiments include systems and methods for removing and recovering residual solvent from a solvent-bearing mass.

FIELD OF THE INVENTION

The present invention relates to recycling solvent, includingefficiently, in terms of recovery percentage, energy expenditure, and/ortime, recovering solvent from a solvent-bearing mass that has undergoneone or more extraction cycles.

BACKGROUND

The processes and apparatuses utilized for solute extraction, such asthe oil extracted from animal or plant-derived material and/or othermasses (e.g., synthetics, pharmaceutically active substances derivedfrom fermentation and/or biosynthesis), typically apply solvent to saidmaterial(s).

Biomass extraction may include the extraction of terpenoids, flavors,fragrances and/or (possibly other) pharmaceutically active ingredientsfrom materials of natural origin. Examples of biomass materials includebut are not limited to flavorsome or aromatic substances such as hops,coriander, cloves, star anise, coffee, citrus peels, fennel seeds,cumin, ginger and other kinds of bark, leaves, flowers, fruit, roots,rhizomes and seeds. Biomass may also be extracted in the form ofbiologically active substances such as pesticides and pharmaceuticallyactive substances or precursors thereto, obtainable e.g., from plantmaterial, a cell culture or a fermentation broth.

Biomass also may include, but are not limited to terpenoids (e.g.,cannabinoids and terpenes), flavonoids, and/or other components from (1)cannabis, hemp, and/or derivatives thereof (e.g., hash, sift kief, androsin, among other examples) and (2) other botanical substances such asterpenoid-bearing plants and/or fruits and/or extracting psilocin,baeocystin, and/or norbaeocystin from psilocibe mushrooms and/orderivatives thereof.

Example solvents include carbon dioxide, hydrocarbon(s), ethanol andmixture thereof. For example, a hydrocarbon solvent may include at leastone of Isobutane, N-Butane, and/or propane solvent. Other possiblesolvents may include the family of solvents based on organichydrofluorocarbons that contain carbon, hydrogen, and fluorine.

There are known techniques for removing solvent residues from asolvent-bearing mass (e.g., biomass) after, for example, a solid-liquidextraction. Ethanol operators utilize centrifugal separators to spin thesolvent-bearing mass at high speeds for recovering residual ethanol.

Another technique is evacuating and heating (e.g., with a heatingjacket) extraction vessel 11, which may remove some residual solvent inthe solvent-bearing mass. This method may have significant drawbacks.For example, poor heat penetration at the core of the solvent-bearingmass can occur, thereby resulting in uneven heating, leaving the core“solvent soaked”, but the sections near the vessel wall thermallydegraded or otherwise befouled.

FIG. 2 shows a “steam-based”, prior-art method for removing residualsolvent, as described in U.S. Pat. No. 6,685,839. Solvent is introducedto the packed bed 12 of biomass within extraction vessel 11 via inlet13. The solvent passes upwards through the biomass, contacts it, andentrains with biomass extract. The solvent-extract mixture is conveyedvia outlet 14 and delivery line 15 to, for example, the remainder of theextraction circuit of FIG. 1.

Steam is supplied via line 19 and flow control valve 17 to which boththe solvent line 18 and steam line 19 are connected. Steam line 19includes an optional drain valve 27 for draining fluid from line 19.Recycle line 26 may recycle steam multiple times through vessel 11.

A flow control valve 20 operably connects outlet 14 to steam line 23 fordelivering solvent-entrained steam to a separator that is in the form ofa hollow container 24. Said container 24 includes an adsorbent materialsuch as activated carbon for absorbing or otherwise separating solventfrom the steam. The container 24 includes an outlet 25, remote from line23, for steam to reach a condenser (not shown) and, in liquid form, toan effluent drain or reservoir.

A disadvantage to this technique is that it requires a furtherseparation step for removing solvent vapor from the mixture of solventand steam or water.

As such, the above systems may be improved upon and examples of new anduseful systems and methods that are relevant to the needs in the fieldare discussed below.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic view of a known closed-loop extraction circuit;and

FIG. 2 is a schematic view of a known apparatus for removing residualsolvent from a solvent-bearing biomass;

FIG. 3 is a schematic view of a known extraction vessel system;

FIG. 4 is a schematic view of a known extraction system;

FIGS. 5-1 and 5-2 are schematic views of a known electric jacket;

FIG. 6 is a schematic view of an extraction system;

FIG. 7 is a schematic view of an extraction vessel;

FIGS. 8-1, 8-2, 8-3, and 8-4 are cross-sectional views of an extractionvessel;

FIGS. 8-5 and 8-6 are cross-sectional views of an extraction vesselcartridge;

FIGS. 8-7, 8-8, and 8-9 are cross-sectional views of an extractionvessel;

FIGS. 9-1 and 9-2 are cross-sectional views of an extraction vessel oran extraction vessel cartridge;

FIGS. 9-3 and 9-4 are cross-sectional views of an extraction vessel;

FIG. 10 is an extraction vessel schematic diagram showing differentstages of residual solvent removal;

FIGS. 11-1, 11-2, 11-3, and 11-4 are cross-sectional diagrams showingdifferent stages of residual solvent removal;

FIGS. 12, 13, 14, 15, 16-1, and 16-2 show various methods andsub-methods for removing residual solvent from a solvent-bearing mass;and

FIGS. 17, 18, and 19 are schematic views of extraction systems.

SUMMARY

According to a first aspect, the disclosure relates a method ofoperating an extraction system for recovering solvent fromsolvent-bearing mass. The method comprises (1) introducing, into anextraction vessel containing at least the solvent-bearing mass, a firstheated fluid portion into a first input orifice of the extractionvessel, the first heated fluid portion having a first temperature thatis at least equal to a first solvent boiling point temperature; (2)evaporating, by the first heated fluid portion, a first liquid solventportion from the solvent-bearing mass, thereby producing a first solventvapor portion; (3) collecting at least the first solvent vapor portionafter exiting a first output orifice of the extraction vessel; and (4)at least substantially containing, during the collecting the at leastthe first solvent vapor portion step, the first heated fluid portionwithin the extraction vessel. One advantage is time efficiently removingresidual solvent while at least substantially maintain separationbetween the heated fluid portion and the solvent vapor portion. It maybe particularly advantageous for large-diameter extraction vessels inmore evenly stripping residual solvent throughout the solvent-bearingmass, including the core of said mass.

In a first possible implementation form of the first aspect of thedisclosure, the solvent-bearing mass including solvent-bearing biomass.Said biomass, after stripped of residual solvent is therefore safer totransport, dispose of, or use in a derivative product. In a secondpossible implementation form of the first aspect or the firstimplementation form, the method further comprises substantiallymaintaining the first heated fluid portion at at least the firsttemperature as the first heated fluid portion travels through at least aportion of the extraction vessel that contains the solvent-bearing mass.Maintaining the heated fluid portion at the first temperature mayprevent, for example, premature condensation of the heated fluidportion. In liquid heated fluid embodiments, maintaining the heatedfluid portion at the first temperature may be advantageous forcontinuing to thermally drive residual solvent from the extractionvessel.

In a third possible implementation form of the second implementationform, the substantially maintaining step comprising heating, during theevaporating the first liquid solvent portion step, at least one of theextraction vessel and an operably coupled extraction system componentthereof for maintaining the first heated fluid portion at at least thefirst temperature.

In a fourth possible implementation form of the first aspect or any ofthe above implementation forms thereof, the at least substantiallycontaining step comprises closing at least the first output orificebefore the first heated fluid portion exits the extraction vessel. Thatcan help substantially maintain the heated fluid portion within anextraction vessel. In a fifth possible implementation form of the firstaspect or any of the above implementation forms thereof, the at leastsubstantially containing step comprises condensing the first heatedfluid portion and thereby producing a first liquid portion. This mayhelp maintain the (formerly) heated fluid portion within an extractionvessel or allow for gravity-assisted draining of the condensed fluidportion. In a sixth possible implementation form of the fifthimplementation form, the condensing step comprises at least one ofincreasing a pressure within the extraction vessel, decreasing atemperature within the extraction vessel, and condensing the firstheated fluid portion by a cold trap that is arranged above and/ordownstream of the extraction vessel.

In a seventh possible implementation form of the first aspect or any ofthe above implementation forms thereof, the method further comprisingmonitoring, by a controller, at least one of a pressure and temperatureof the extraction vessel. In an eighth possible implementation form ofthe seventh implementation form, the monitoring step comprises measuringat least one extraction vessel temperature with at least one thermalsensor arranged on or in the extraction vessel. In some embodiments, acontroller can use the measured temperature values to determine avapor-pressure value or an average thereof. In a ninth possibleimplementation form of the seventh or eighth implementation forms, themonitoring step comprises monitoring a thermal gradient value across alength of the extraction vessel. In some embodiments, the gradient valuemay indicate the progress of the first heated fluid portion as itascends or descends through an extraction vessel.

In a tenth possible implementation form of the seventh, eight, or ninthimplementation forms, the first input orifice is arranged on or near afirst end portion of the extraction vessel and the first output orificeis arranged on or near a second end portion of the extraction vessel,with the first and second end portion arranged on opposite ends of theextraction vessel. The monitoring step comprises monitoring, by thecontroller, at least a temperature of the second end portion of theextraction vessel. In some embodiments, the monitored temperature mayindicate that the first heated fluid portion may be close to exiting anextraction vessel.

In an eleventh possible implementation form of the seventh, eight,ninth, or tenth implementation forms, the method further comprises atleast substantially stopping, possibly by the controller, theintroduction step in response to a first monitored value that isobtained from the monitoring stop, the first monitored value comprisingat least one of a first extraction vessel pressure value, a firstextraction vessel temperature value, and a first extraction vesselthermal gradient value. One advantage may be substantially maintainingseparation between the heated fluid portion and the solvent vaporportion by preventing the heated fluid portion from overflowing theextraction vessel.

In a twelfth possible implementation form of the seventh, eighth, ninth,tenth, or eleventh implementation forms, the method further comprisesclosing, possibly by the controller, the extraction vessel in responseto a second monitored value that is obtained from the monitoring step,the second monitored value comprising at least one of a secondextraction vessel pressure value, a second extraction vessel temperaturevalue, and a second extraction vessel thermal gradient value. Oneadvantage may be at least substantially maintaining separation betweenthe heated fluid portion and the solvent vapor portion.

In a thirteenth possible implementation form of the first aspect or anyof the above implementation forms, the method further comprisesmonitoring, possibly by the controller, a vapor pressure of theextraction vessel; and determining, possibly by a controller, if amonitored vapor pressure value indicates that residual solvent remainsin the extraction vessel. If it is determined that residual solventremains in the extraction vessel, the method further comprising (1)introducing a second heated fluid portion into the first input orificeor another input of the extraction vessel; (2) substantially maintainingthe second heated fluid portion in vapor form as the second heated fluidportion travels through the extraction vessel; (3) evaporating, by thefirst heated fluid portion, a second liquid solvent portion from thesolvent-bearing mass, thereby producing a second solvent vapor portion;(4) collecting at least the second solvent vapor portion after exitingthe first output orifice of the extraction vessel; and (5) at leastsubstantially containing the second heated fluid portion within theextraction vessel. One advantage is a thorough removing residualsolvent.

In a fourteenth possible implementation form of the thirteenthimplementation form, the method comprises sealing, possibly by acontroller, the extraction vessel or a fluidly coupled path thereofbefore determining if the monitored vapor pressure value indicates thatresidual solvent remains in the extraction vessel. One advantage isisolating the extraction vessel when determining if residual solventstill remains in said vessel.

In a fifteenth possible implementation form of the first aspect or anyof the above implementation forms thereof the solvent-bearing masscomprises at least two solvents with differing boiling pointtemperatures, including the first solvent boiling point temperature anda second solvent boiling point temperature. The method further comprises(1) introducing a second heated fluid portion into the first inputorifice or another input of the extraction vessel, the second heatedportion being at a higher temperature than the first heated fluidportion and at least equal to the second solvent boiling point; (2)evaporating, by the second heated fluid portion, a second liquid solventportion from the solvent-bearing mass, thereby producing a secondsolvent vapor portion; (3) collecting at least the second solvent vaporportion after exiting the first output orifice of the extraction vessel;and (4) at least substantially containing the second heated fluidportion within the extraction vessel. One advantage is the ability toevaporate selected solvent(s) at a time, in isolation (e.g., onlybutane) or in a particular “grouping” (e.g., butane and isobutane).Solvents can then be separately stored for later use, eitherindividually or in sub-groupings, without further separation steps.

In a sixteenth possible implementation form of the first aspect or anyof the above first through fourteenth implementation forms thereof, thesolvent-bearing mass comprises at least two solvents with differingboiling point temperatures, including the first solvent boiling pointtemperature and a second solvent boiling point temperature that ishigher than the first solvent boiling point temperature. The (1)introducing the first heated. fluid portion step comprises introducing,into the extraction vessel, the first heated fluid portion into thefirst input orifice of the extraction vessel, the first heated fluidportion having the first temperature that is at least equal to thesecond solvent boiling point temperature; and the (2) evaporating stepcomprising evaporating, by the first heated fluid portion, the firstliquid solvent portion from the solvent-bearing mass, thereby producingthe first solvent vapor portion that comprises the at least twosolvents. One advantage is the ability to evaporate a group of solventsin a time-efficient manner.

In a seventeenth possible implementation form of the first aspect or anyof the above implementation forms thereof, the introducing the firstheated portion step comprising introducing, into the extraction vessel,a first heated vapor portion into the first input orifice of theextraction vessel.

In an eighteenth possible implementation form of the first aspect or anyof the above implementation forms thereof, the method further comprisesevacuating, before introducing the first heated fluid portion, asolvent-solute mixture from the extraction vessel while retaining thesolvent bearing mass within the extraction vessel.

In a nineteenth possible implementation form of the first aspect or anyof the above implementation forms thereof, the method further comprisesevacuating, after at least the evaporating the first liquid solventportion step, at least one of the first heated portion and a liquidportion thereof from the extraction vessel. In a twentieth possibleimplementation form of the nineteenth implementation form, theevacuating the first heated portion step comprises heating, after atleast the evaporating the first liquid solvent portion step, theextraction vessel to at least a fluid portion boiling point forevaporating at least one of the first heated fluid portion and theliquid portion thereof.

In a twenty-first possible implementation form of the first aspect orany of the above implementation forms thereof, the first heated fluidportion comprises at least one of a heated gas, heated CO2, heatedliquid water, and water vapor. In a twenty-second possibleimplementation form of the first aspect or any of the aboveimplementation forms, the solvent-bearing mass comprises at least one ofethane, propane, ammonia, water, xenon, methanol, ethanol, 1-propanol,2-propanol, 1-hexanol, 2-methoxy ethanol, tetrahydrofuran, 1,4-dioxane,acetonitrile, methylene chloride, dichloroethane, chloroform, ethylacetate, propylene carbonate, N,N-dimethylacetamide, dimethyl sulfoxide,formic acid, carbon disulfide, acetone, toluene, hexanes, pentanes,trifluoromethane, nitrous oxide, sulfur hexafluoroide, butane,isobutane, ethyl ether, benzotrifluoride, (p-chlorophenyl)trifiuoromethane, chlorofluorocarbon (CFC), hydrofluorocarbon, HFA-134a,terpenes, terpenoids, or a mixture thereof.

According to a second aspect, the disclosure relates to a method ofthermally regulating an extraction vessel. The method comprises (1)introducing, into the extraction vessel containing at least asolvent-bearing mass, a first thermally regulated fluid portion into afirst plurality of input orifices of the extraction vessel, each of thefirst plurality of input orifices partially defining an extractionvessel channel for transporting fluid along a length of the extractionvessel without the thermally regulated fluid contacting thesolvent-bearing mass; and (2) thermally regulating, by the firstthermally regulated fluid portion, a first liquid solvent portion incontact with the solvent-bearing mass. One advantage may be an“internal” thermal regulator, which may be able to thermally regulatethe core of a solute- and/or solvent-bearing mass in, for example, alarge-diameter extraction vessel. Said thermal regulation may occurbefore, during, or after solute extraction within the extraction vessel.

According to a third aspect, the disclosure relates to a method ofrecovering solvent from solvent-bearing mass. The method comprises (1)introducing, into an extraction vessel containing at least thesolvent-bearing mass, a first heated fluid portion into at least a firstinput orifice of the extraction vessel, the first heated fluid portionhaving a first temperature that is sufficient to establish or increase apressure within the extraction vessel; (2) moving, by the first heatedfluid portion, at least a first liquid solvent portion from thesolvent-bearing mass, thereby producing a first evacuated solventportion; (3) collecting at least the first evacuated. solvent portionafter said portion exits a first output orifice of the extractionvessel; and (4) at least substantially containing, during the collectingthe at least the first evacuated solvent portion step, the first heatedfluid portion within the extraction vessel. One advantage may beremoving residual solvent at relatively lower temperatures by relying onthermally driving the residual solvent out of the extraction vessel.

According to a fourth aspect, the disclosure relates to an extractionvessel comprising an elongated vessel defining at least a first exteriorshape and an interior cavity; and a plurality of protrusions that (A)are arranged within the elongated vessel, (B) extend into the cavity,and (C) are thermally coupled to the elongated vessel. In a firstpossible implementation form of the fourth aspect, the plurality ofprotrusions comprise a plurality of fins that (A) are arranged withinthe elongated vessel, (B) extend into the cavity, and (C) are thermallycoupled to the elongated vessel. One advantage may be an “internal”thermal regulator, which may be able to thermally regulate the core of asolute- and/or solvent-bearing mass in, for example, a large-diameterextraction vessel.

In a second possible implementation form of the fourth aspect or firstimplementation form, the plurality of protrusions each substantiallyspan a length of the elongated vessels. In a third possibleimplementation form of the fourth aspect or the above implementationforms thereof, each of the plurality of protrusions ate mechanicallycoupled to the elongated vessel. One advantage may include selectingdifferent materials for the protrusions than for the extraction vesselexterior.

In a fourth possible implementation form of the fourth aspect or theabove implementation forms thereof, the extraction vessel furthercomprises a thermal jacket that is thermally coupled to at least theplurality of protrusions. In a fifth possible implementation form of thefourth implementation from, the thermal jacket mechanically couples toan exterior portion of the elongated vessel. In a sixth possibleimplementation form of the fourth or fifth implementation forms, thethermal jacket is one of a liquid jacket and an electric jacket.

In a seventh possible implementation form of the fourth aspect or theabove implementation forms thereof, the plurality of protrusions eachcomprise one or more heating elements. In an eighth possibleimplementation form of the fourth aspect or the above implementationforms thereof, the plurality of protrusions each comprise one or moreresistive heating elements.

In a ninth possible implementation form of the fourth aspect or thesecond through sixth implementation forms thereof, the plurality ofprotrusions each define a cavity for transporting a heating fluid and/orcooling fluid across a length of the extraction vessel.

In a tenth possible implementation form of the fourth aspect or theabove implementation forms thereof, the plurality of protrusions eachcomprise a ferrous material. One possible advantage is the ability toutilize an inductive heating source to heat the plurality ofprotrusions.

According to a fifth aspect, the disclosure relates to an extractionvessel system that comprises any one of the extraction vessels of thethird aspect and implementation forms thereof. The system furthercomprises an extraction vessel cartridge adapted to hold a sourcematerial for extraction, with the cartridge dimensioned and defining acomplementary shape and thereby configured to slide into the extractionvessel.

According to a sixth aspect, the disclosure relates to an extractionvessel system that comprises any one of the extraction vessels of thethird aspect and implementation forms thereof besides the fourth throughsixth implementation forms. The system further comprises a thermaljacket operably coupled or integral with the extraction vessel, thethermal jacket arranged to be thermally coupled with or otherwise heatat least the protrusions.

According to a seventh aspect, the disclosure relates to an extractionvessel system that comprises an extraction vessel and an extractionvessel cartridge. The extraction vessel cartridge comprises a ferrousmaterial and is adapted to hold a source material for extraction. Thecartridge is dimensioned and defines a complementary, shape and isthereby configured to slide into the extraction vessel. One possibleadvantage is the ability to utilize an inductive heating source to heatthe cartridge, inside the extraction vessel, for the thorough removal ofresidual solvent.

According to an eighth aspect, the disclosure relates to an extractionsystem that comprises a controller that is configured or configurable toperform at least any one method of the first aspect and implementationforms thereof.

DETAILED DESCRIPTION

The disclosed methods and systems will become better understood throughreview of the following detailed description in conjunction with thefigures. The detailed description and figures provide merely examples ofthe various inventions described herein. Those skilled in the art willunderstand that the disclosed examples may be varied, modified, andaltered without departing from the scope of the inventions describedherein. Many variations are contemplated for different applications anddesign considerations; however, for the sake of brevity, each and everycontemplated variation may not be individually described in thefollowing detailed description.

Throughout the following detailed description, examples of varioussystems are provided. Related features in the examples may be identical,similar, or dissimilar in different examples. For the sake of brevity,related features will not be redundantly explained in each example.Instead, the use of related feature names will cue the reader that thefeature with a related feature name may be similar to the relatedfeature in an example explained previously. Features specific to a givenexample will be described in that particular example. The reader shouldunderstand that a given feature need not be the same or similar to thespecific portrayal of a related feature in any given figure or example.

As used herein, “thermal elements” include elements for applying atleast one of heat or cooling to an object such as thermoelectricelements Peltier devices), thermal liquid jackets (e.g., water jackets),heating elements (e.g., inductive and other resistive heating elements,pads, heaters, stoves), and electric jackets.

Unless otherwise noted, a dotted line that connect two or moreextraction system components in the figures generally signifies one ormore fluid communication paths between or among said two or moreextraction system components. Fluid lines, pumps, valves, and/or furtherextraction system components may he arranged along said fluidcommunication path and may be omitted in the figures for sake of clarityand highlighting inventive aspects. Further, multiple dotted linesbetween extraction components do not necessarily indicate multiplephysical lines arranged between components, but rather different fluidssuch as solvent, solvent mixtures, solvent-solute mixtures, and/or aheated fluid may share one or more lines.

Extraction system components in “fluid communication” means that a fluidcan at least flow from one extraction system component to the other.Extraction system components can still he in fluid communication evenwith intervening pumps, valves, and/or further extraction systemcomponents (e.g., a separator). “Selective fluid communication” meansthat a fluid connection may be selectively established via, for example,a fluid connector (e.g., valves, manifolds, and the like). “Fluidconnector” may include one or more valves such as one-, two, three-,four-way valve(s) and/or manifolds, which generally include a pluralityof valves.

One advantage for various large-diameter (e.g., around twelve inches orlarger) extraction vessels is the thorough removal of residual solvent,thereby decreasing solvent loss and providing a safer by-product (e.g.,a mass after extraction and residual solvent removal) for transport,disposal, or even as a source for another product. Another possibleadvantage is a more flexible solvent-removal process, in which solventmay be selectively evaporated at particular temperatures occurringwithin the extraction vessel. In some embodiments, a heated fluid may beof a sufficient temperature to evaporate a plurality or sub-plurality ofsolvents having differing boiling points.

A further possible advantageous example is monitoring for subsequentpressure signatures or changes within the extraction vessel or elsewherein a fluidly coupled line of one or more extraction system components.Said pressure signature is generally indicative of the mass stillcontaining residual solvent after at least a first residual-solventremoval step.

A further advantage is substantially maintaining the heated fluid (thatevaporates or otherwise displaces the one or more solvents) within theextraction vessel, or additionally or alternatively, arranging a coldtrap downstream, with respect to the flow direction of the heated fluid,of the extraction vessel for condensing a heated vapor and therebypreventing a heated vapor from entering a further extraction systemcomponent. in some embodiments, said condensed fluid (i.e., formerly theheated vapor) returns, with the assistance of gravity, back into theextraction vessel. In cold trap embodiments, the (formerly) heated fluidis “substantially maintained” within the extraction vessel as saidheated fluid (or a portion thereof) only briefly exits the extractionvessel before returning in liquid form.

As shown by FIG. 1, extraction system 101 includes first tank 110,second tank 140, extraction column 11, and an optional pump 150. Solventline 112 a and valve 102 are arranged between first tank 110 andextraction column 11. Liquid mixture line 112 b and valve 104 arearranged between extraction column 11 and second tank 140. Solventrecapture line 112 c, valves 106 and 108, and pump 150 are arrangedbetween second tank 140 and first tank 110. Pressure source 152 (e.g.,an optional tank or optional compressor) can provide or add pressure tofirst tank 110 by providing a pressurized gas, via line 112 d and valve109 for moving or assisting in moving solvent from first tank 110 toextraction column 11.

Thermal elements 111 and 141 are respectively thermally coupled to firsttank 110 and second tank 140. Thermal elements 111 and 141 may beremovably coupled and/or directly mechanically coupled to the exteriorof its respective tank. In one example, thermal elements 111 and 141 arefluid jackets that are respectively welded to first tank 110 and secondtank 140. Thermal elements 111 and 141 may heat and/or cool theirrespective first and second tanks 110 and 140.

FIG. 3 is a schematic view of example extraction system 300, whichincludes support structure 306, extraction cartridge 302, extractionvessel 350, and extraction vessel lid 351, which is mechanicallycouplable to vessel 350 for removing cartridge 302 and establishing aseal for vessel 350. Vessel 350 is generally fixed to support structure306, but may be removeable via tools for replacement or maintenance.Cartridge 302 may be, for example, a rigid mesh “basket” or a deformablemesh “bag” that contains the source material. One example of cartridge302 is a wire-mesh basket. In some examples, the outer surface of saidwire-mesh basket is coated with silicon for directed solvent towards themass held therein.

Thermal elements may include electric jackets, which may includedeformable material for wrapping around an extraction system componentand/or may be pads arranged to abut one side of an extraction systemcomponent, such as the bottom side of a separator vessel. FIGS. 4, 5-1,and 5-2 show a prior art extraction system and electric heating jackets.Solvent vessel 402 is fluidly coupled to extraction vessel 404 with line403. Both vessels 402 and 404 have an electric heating jacket,respectively electric heating jackets 406 and 408. The “back” side ofjacket 408 is shown, which includes straps 408 a engaged with buckle 408b for snugly coupling the deformable material of jacket 408 with theouter surface of vessel 404.

FIG. 5-1 shows electric heating jacket 506 with straps 508 in acylindrical form on its own, without an extraction system component suchas a solvent or extraction vessel. FIG. 5-2 shows the jacket “flattenedout” to show the deformable quality of jacket 506. Straps 508 may couplewith buckles (not shown), Velcro, or other coupling structures forsnugly coupling jacket 508 to an extraction system component.

FIG. 6 shows extraction system 600, which shows controller 602 operablycoupled to memory 602 a, fluid connectors 604 and 606, and at least onethermal sensor 616. The electrical connections among controller 602,thermal sensor 616, and pressure sensor 618 are not shown for overallclarity of FIG. 6. Example operable connections may be wired or wirelesselectrical coupling (e.g., USB, Ethernet (e.g., IEEE 802.3), IEEE.802.11, Bluetooth). Alternatively or additionally, controller may beoperably connected to fluid connectors 604 and 606 via a pneumaticconnection(s) in order to avoid bringing electrical signals near theextraction process.

Sensor(s) 616 may be arranged on and/or within extraction vessel 611.Sensors 616 and/or 618 may be arranged within vessel 611 as probesensors. In multiple thermal sensor embodiments, sensors 616 may bearranged along a length of extraction vessel 611 and thereby measuring,for example, thermal gradients along said length and otherlocation-related temperature values. In such embodiments, sensors 616may provide measurements at different local areas for tracking theprogress of a heated fluid. as it travels through extraction vessel 611for thermally moving solvent via a heated liquid or vapor. Controller602 can thereby “track” or monitor the progress of the heated fluid fromheated fluid source 610.

Heated fluid source 610 may be a tank or other vessel that is thermallycoupled to heating element 608, which may be operably coupled tocontroller 602 for controlling the application of heat to source 610.

Solvent source 615 may provide solvent to the top, side, and/or bottomof vessel 611 for extraction. FIG. 6 shows solvent source 615 arrangedto fluidly communicate solvent to vessel 611 via connector 604 to“top-fill” said vessel 611, but bottom-filling and side-filling, mayoccur additionally or alternatively.

After an extracting time period, the resultant solvent-solute mixturemay be evacuated out of vessel 611, to separator 619 for separatingsolute from solvent. The solute may then flow to extract container 622and solvent vapor to source 615 or to another solvent container.

After a solvent-solute evacuation step, a solvent-bearing mass remainsin vessel 611.

Controller 602 may direct a heated fluid (liquid or gas) from heatedfluid source 610 to vessel 611 via fluid connector 606. Controller 602may then monitor the progress of the heated fluid. Said heated fluid mayalternatively be introduced via a side or top of extraction vessel 611.

As shown in FIGS. 6, 10, and 11, the heated fluid may rise through thecolumn. Said heated fluid may gently remove solvent via displacement.That is, a heated liquid, for example, may cause residual solvent to bethermally driven such that the solvent remains, for example, in liquidform as it exits vessel 611.

In another technique, the heated fluid may be at least a boiling pointtemperature of the solvent. In such embodiments, the residual solvent isevaporated and may flow to an optional condenser 614 and then to source615 or another vessel. In some embodiments, source 615 may be the firstcondensing element that the vapor reaches (e.g., condensed via a cooledsolvent tank).

Controller 602 may allow the heated fluid to progress to or near the topof vessel 611. As controller 602 monitors the progress, it may dosefluid connector 604 and/or 606 in response to sensor 616 reaching orpassing a certain temperature value. Said temperature value may be atarget temperature for removing residual solvent and/or a temperaturedifferential value between two or more sensors 616.

For example, controller 602 may dose connectors 604 and 606 in responseto a value based on at least value from one or more sensors 626. Then,pressure sensor 618 may be monitored, by a user and/or controller 602,to determine if a pressure value indicates that residual solvent yetremains in the (still) solvent-bearing mass. As explained below in moredetail, a pressure signature value may be a vapor pressure value or anaverage thereof. In some embodiments, the pressure signature may includea raise in pressure beyond a threshold value, particularly inembodiments that fluidly isolate vessel 611 and monitor the pressure ofthe isolated vessel 611. However the pressure signature is monitored,said signature indicates that residual solvent remains, and furtherheated fluid may be introduced.

The heated fluid may he introduced multiple times at multipletemperature for recovering multiple solvents with differing boilingpoints. For example, the heated fluid may be applied and removed at aboiling point temperature for each solvent type that resides within thesolvent-bearing mass.

During or after the residual-solvent removal process, the heated fluidmay be evacuated from vessel 611 to source 610. Heated vapor (e.g.,steam) may he condensed within vessel 611 into a liquid before beingtransported back to source 610 or another vessel. In some embodiments,the condensed liquid's flow may be gravity assisted as it travelstowards source 610.

Thermal element 612 may be thermally coupled to vessel 611 for coolingand/or heating the heated fluid. Thermal element may be a liquid jacket,an electrical jacket, or a Peltier device adapted to both heat and coolextraction vessel 611. In some embodiments, thermal element includes aninductive jacket for inductively heating one or more elements arrangedwithin vessel 611, such as fins, protrusions, an extraction vesselcartridge that comprise at least one ferrous material.

Control 602 may thermally regulate heated fluid by applying heat,electrically and/or fluidly, to maintain at least a solvent boilingpoint temperature, cooling to condense said heated liquid, and/or heatequal at least a heated fluid boiling point temperature to assist inevacuating the heated fluid.

In general, system 600 is adapted, via controller 602, human operation,or a combination, to at least substantially maintain the heated fluidwithin vessel 611 during the residual solvent removal step(s). As such,the liquid or vapor-form solvent is generally free of the heated liquid,thus simplifying the solvent recovery process. Alternatively oralternatively, a cold trap may reside, for example, immediatelydownstream of an output orifice of vessel 611. In some embodiments, thecold trap's temperature condenses the (formerly) heated vapor into aliquid, but passes solvent vapor, which condenses at a lowertemperature. Said cold trap may gravity feed said output orifice ofvessel 611, thereby re-directing the liquid fluid back into vessel 611and thereby substantially maintaining the fluid within the extractionvessel as system 600 only briefly allows perhaps some of the heatedvapor to exit, but it is condensed and flowed back into vessel 611.

FIG. 7 shows extraction vessel system 700, which includes extractionvessel 611 with a plurality of thermal sensors 616, pressure sensor 618,input orifice 702, output orifice 704, and at least one thermal element612. At least one thermal element 612 a may be arranged on or near amid-section of vessel 611 for thermally regulating at least the heatedfluid. One example of thermal regulation is maintaining at least asolvent boiling point temperature.

The thermal element(s) 612(b) may also be arranged to cool heated vapor(as the heated fluid) for condensing said vapor within vessel 611 In oneexample, the condensation temperatures of the heated vapor and theresidual solvent vapor may be sufficiently far apart such that the vaporcondenses in the top portion of vessel 611, but the solvent vapor passesthrough. In another example, thermal element 612(b) cools the heatedvapor after most of the residual solvent has exited vessel 611, butbefore the heated vapor reaches output orifice 704.

As explained in more detail, thermal element(s) 612 a and 612 b may bethermally coupled to fins or other internal features for ensuring a coreof the solvent-land mass reaches at least a solvent boiling pointtemperature. Thermal elements 612 a and 612 b may be arranged on anexterior of vessel 611 and said fins or other features arranged on ordefining an interior of vessel 611.

FIGS. 8-1 and 8-2 show two possible cross sections of vessel 611 takenalong line A of FIG. 6 and/or 7. In general, all non-circular cavity 611i shape variations fall within the scope of the innovations. In FIG.8-1, vessel 611 includes exterior 611 a and interior 611 b. Interior 611b defines a star-shaped cavity 611 i and include protrusion 611 j withpeaks 611 p and recesses 611 c. FIG. 8-2 similarly defines anon-circular cavity 611 i, which may be characterized as a ninja staror, more generally, a four-pointed star.

Protrusions 611 j may be integral with interior 611 b or maymechanically coupled to vessel 611 via welding or other techniques fordefining non-circular cavity 611 i. For example, as seen in FIGS. 8-3and 8-4, joint 611 k may couple protrusions 611 j with vessel 611 via anotch defined on each protrusion. In alternative embodiments, joint 611k may comprise a tail defined by protrusion 611 j that dovetails with anotch of vessel 611 (e.g., 611 n of FIGS. 9-3 and 9-4).

Protrusions 611 j may be passive such that it thermally couples asolvent-bearing mass with a thermal element that resides outside ofcavity 611 i (e.g., an electric or liquid jacket). Possible passiveexamples include thermally conductive metals (e.g., copper) and ferrousand non-ferrous materials.

In ferrous-material embodiments, protrusions 611 j may be operablycoupled to an induction source (e.g., an inductive jacket). Theinduction source may be adapted to heat protrusions 611 j to adistillation temperature for distilling one or more solvents and/orcomponents such as terpenes, flavonoids, and/or cannabinoids (e.g.,THC).

For example, a jacketed coil of wire (not shown) may be operably coupledto vessel 611 and an alternating electric current is passed through saidwire. The resulting oscillating magnetic field wirelessly induces anelectrical current in one or more protrusions 611 j. This induced eddycurrent that flows through the protrusions 611 j results in heating ofthe solvent-bearing mass or material.

Alternatively or additionally, protrusions 611 j may encompass heatingelement 611 h, which may be a resistance heating feature running along alength of vessel 611 such as an electrical wire arranged and adapted toheat protrusion 611 j. FIGS. 8-7, 8-8, and 8-9 show a plurality oforifices 611 o arranged and adapted to thermally regulate vessel 611 viaa thermally regulated fluid, typically for heating or cooling anextraction vessel before, during, or after an extraction process. Saidorifices 611 o partially define a channel that extends along a length ofvessel 611. Said channel(s) (e.g., 611 t of FIG. 19) are physicallyseparated from cavity 611 i, thereby preventing any mixture of athermally regulating fluid with the solvent that resides within cavity611 i. Said channel(s) (e.g., 611 t of FIG. 19) may partially define acircuit for flowing thermally regulated fluid.

FIGS. 8-5 and 8-6 show a cross section of extraction vessel cartridge811, which is similar to the cartridge 302 shown in FIG. 3, but anon-cylindrical shape for dovetailing with non-circular cavity 611 i ofvessel 611. Said cartridge 811 is typically loaded up with a sourcematerial and then slid into vessel 611. Cartridge 302 may be, forexample, a rigid mesh “basket” that contains the source material, butalso allows solvent and other fluids to pass through.

Cartridge 811 includes exterior 811 a, interior 811 b, peak 811 p,recessed 811 c, and cavity 811 i.

FIGS. 9-1 and 9-2 show two further possible cross sections of vessel 611taken along line A of FIG. 6 and/or 7 or an extraction cartridge vesselcartridge 911 similar to cartridge 302, but further comprising aplurality of fins 911 c, 911 d. In other words, a plurality of fins 911c or 911 d may be arranged on extraction vessel 611 or cartridge 911. Ineither case, a plurality of fins resides within extraction vessel 611for thermally coupling with a solvent-hearing mass.

Exterior 611 a, 911 a may define a generally circular shape. Interior611 b, 911 b may be generally define a circular cavity 611 i, 911 i andhave one or more fins 911 c and 911 d arranged within it. Said fins mayeach encapsulate (or define) a resistant heating element (e.g., Jouleheating) for directly heating a solvent-bearing mass, with or withoutassistance from a heated fluid and/or an exterior thermal element suchas a liquid jacket. That is, fins 911 c and 911 d may actively heat viaan electrical signal or passively heat via an external heating elementthat is thermally coupled to said fins 911 c and 911 d. Other shapedfins are within the scope of the innovations as FIGS. 9-1 and 9-2 showonly two example shapes: tapered fin 911 d and non-taped fin 911 c.

For example, fins 911 c and 911 d may be thermally coupled to a liquidjacket and thereby transfer heat from interior 611 b towards the core ofa solvent-hearing mass. Said fins 911 c and 911 d may be mechanicallycoupled to interior 611 b. In one example, each fin 911 c/ 911 d may bewelded onto interior 611 b. The length of each fin may span the lengthof vessel 611 or only a section thereof (e.g., only a mid-section ofvessel 611).

Alternatively or additionally, fins 911 c and 911 d may comprise aferrous material that is arranged and adapted to be heated via inducededdy currents (e.g., inductive heating). Alternatively or additionally,cartridge 911 or a circular-cross-section cartridge may comprise aferrous material that are arranged and adapted to be heated via inducededdy currents. In some embodiments, exterior 611 a and/or exterior 611 bcomprise a non- or weakly (e.g., weakly ferromagnetic) ferrous material.

FIGS. 9-3 and 9-4 show two further possible cross sections of vessel 611taken along line A of FIG. 6 and/or 7. Interior 611 b defines aplurality of notches 611 n for coupling with a respective plurality ofprotrusions such as fins 911 c, 911 d, and/or protrusions 611 j.Alternatively, a protrusion (e.g., fins 911 c, 911 d and/or protrusions611 j) may define a notch that couples with a coupling protrusiondefined by interior 611 b.

FIG. 10 shows changes in the thermal gradient as the heated liquid, inthis example, raises from the bottom of vessel 611 to near a tope ofvessel 611. In some embodiments, a gradient “length” is measured by aplurality of thermal sensors such that a controller, in response to thelength passing or matching a threshold value, will close at least onefluid connector to (1) stop the introduction of the heated fluid intovessel 611; (2) stop the heated fluid from leaving vessel 611; (3) orboth (1) and (2). A gradient length may be defined as the distancebetween an upper edge of a relatively uniform heated section and anopposing cold section or other end point.

In some embodiments, a gradient is not considered, but rather a localtemperature near a top section of vessel 611 matching or passing atemperature value, indicative of the heated liquid occupying acorresponding area within the extraction vessel 611 and, in response, acontroller performs one or more of the above mention steps (1) and (2).For example, as seen at T3, vessel 611 includes an internal temperaturesensor 616 dimensioned and arranged to detect a heated fluid temperatureat location that allows for a controller to close an exit fluidconnector before the heated liquid leaves vessel 611 and/or stop thesupply of heated liquid by closing an entrance fluid connector of vessel611.

FIGS. 11-1 to 11-4 shows this process in more detail via a schematiccross sectional sideview of vessel 611. At a first stage of the residualsolvent recovery process, a heated fluid may flow through perforateddisc 1104 for possibly a more even redistribution of the flow of apossibly pressurized heated fluid that flows from input orifice 702.Said disc 1104 may prevent channeling of the heated fluid as it passesthrough solvent-bearing mass 1101.

At this point of the solvent recovery process, boundary layer 1106 showsa dividing line between the leading edge of the rising heated fluid assaid fluid proceeds to move up extraction vessel 611. At this point, theheated fluid occupies area 1102, which includes only a bottom section ofvessel 611. Although the heated fluid is showing a “bottom-filling”environment, heated fluids may be alternatively side-loaded ortop-loaded.

The heated fluid causes solvent 1103 to flow upward. In someembodiments, solvent 1103 may substantially retain a liquid state. Inother embodiments, solvent 1103 may be substantially solvent vapor, withthe heated fluid being, at least a solvent boiling point temperature. Insome embodiments, the heated fluid may be substantially above saidboiling point temperature.

FIG. 11-2 shows vessel 611 at a later stage of the residual solventrecovery process. Area 1102 has increased and boundary layer 1106 hasrisen to be closer to output orifice 704, which is passing solvent 1103that is “pushed out” by heated fluid. That is, residual solvent 1103exits extraction vessel 611.

FIG. 11-3 shows vessel 611 at an even later stage of the residualsolvent recovery process. Area 1102 has increased and boundary layer1106 has risen to be near output orifice 704. At this point in time (orsoon thereafter) output orifice 704 is closed for blocking the heatedfluid from exiting vessel 611. After sealing vessel 611, includingpossibly closing input orifice 702, an extraction vessel pressure may bemonitored to determine if there is a significant amount of residualsolvent remaining.

FIG. 11-4 shows vessel 611 at a late stage of the residual solventrecovery process. Area 1102 had increased and boundary layer 1106 hasrisen to be near output orifice 704. Thermal element 612 b cools the topsection of vessel 611 for producing condensed portion 1105, whichcomprises condensed fluid, but passes solvent 1103 in vapor form. Inother words, thermal element 612 b at least substantially retains heatedfluid within vessel 611 by condensing, for example, water vapor; butpassing hydrocarbon solvents, which have much lower condensingtemperatures.

FIG. 12 shows a method for recovering solvent from solvent-bearing mass.Step 1202 includes introducing, into an extraction vessel containing atleast the solvent-bearing mass, a first heated fluid portion into afirst input orifice of the extraction vessel, the first heated fluidportion having a first temperature that is at least equal to a firstsolvent boiling point temperature. Step 1204 a includes evaporating, bythe first heated fluid portion, a first liquid solvent portion from thesolvent-bearing mass, thereby producing a first solvent vapor portion.Optional step 1205 includes heating, during the evaporating step 1204 a,the extraction vessel or an operably coupled extraction componentthereof (e.g., fins or protrusions) for maintaining the first heatedfluid portion at at least the first temperature. Said heating mayinclude a liquid jacket, electric jacket, resistive heating elements,among other examples, applying heat to an extraction vessel or directlyto a solvent-bearing mass.

Step 1206 includes collecting at least the first solvent vapor portionafter exiting a first output orifice of the extraction vessel. Step 1208includes at least substantially containing, &ring the collecting the atleast the first solvent vapor portion step 1206, the first heated fluidportion within the extraction vessel. Step 1210 include evacuating,after at least the evaporating the first liquid solvent portion step1204 a, the first heated portion and/or a liquid portion thereof fromthe extraction vessel. Said evacuation may be pressure-, thermal-,gravity-, and/or vacuum-assisted. For example, a pressure source mayforce out the heated portion (an example of pressure-assistedevacuation). The heated portion may be vapor, liquid., or a combinationthereof. In some embodiments, the heated portion is condensed within theextraction vessel before evacuation. Thermal-assisted embodiments Maudeheating the heated portion to its boiling point temperature to evacuatea vapor or condensing the heated portion to evacuate a liquid from theextraction vessel.

FIG. 13 shows a sub-method for recovering solvent from solvent-bearingmass in which step 1208 a includes condensing, during the collecting theat least the first solvent vapor portion step 1206, at least asub-portion of the first heated fluid portion within the extractionvessel and thereby producing a first liquid portion.

FIG. 14 shows a sub-method for recovering solvent from solvent-bearingmass in which step 1210 includes evaporating, by a second heated fluidportion, a second liquid solvent portion from the solvent-bearing mass,thereby producing a second solvent vapor portion.

FIG. 15 shows a sub-method for recovering solvent from solvent-bearingmass in which step 1202 a includes introducing, into an extractionvessel, a first heated fluid portion into a first input orifice of theextraction vessel, the first heated fluid portion having a firsttemperature that is at least equal to a solvent boiling pointtemperature that is sufficient to evaporate at least a sub-plurality ofsolvents. Step 1204 b includes evaporating, by the first heated fluidportion, a first liquid solvent portion comprising at least thesub-plurality of solvents, thereby producing a first solvent vaporportion.

FIG. 16-1 shows a sub-method for recovering solvent from solvent-bearingmass. Step 1207 a includes maintaining an extraction vessel at a solventboiling-point temperature. Said temperature may be monitored with athermal sensor arranged inside and/or an exterior surface of anextraction vessel.

Step 1209 a includes monitoring at least an extraction vessel pressure.Said pressure may be monitored with a pressure sensor (e.g., a probeand/or gauge) that is operably coupled to the extraction vessel. In thisexample, “after step 1204 a” of step 1209 a merely specifies aparticular instance of when pressure monitoring is occurring, but notnecessarily when said monitoring is initiated. For example, a pressuremay be monitored by a controller or human operator before, during,and/or after most steps.

Step 1212 includes evaporating further residual solvent that remains inan extraction vessel if the monitored pressure indicates that residualsolvent remains in the solvent-bearing mass. One example embodiment ofstep 1209 a includes monitoring a sealed extraction vessel that ismaintained at at least a solvent boiling point temperature. In general,if residual solvent remains within an extraction vessel, a vaporpressure (gauge) value will match a vapor pressure signature of saidresidual solvent while the extraction vessel is maintained at a solventboiling point temperature of a particular solvent or a mixture thereof.Example embodiments include detecting a particular pressure thresholdvalue or change in pressure value with respect to a previously measuredpressure value (e.g., pressure values from before and after sealing ofthe extraction vessel).

FIG. 16-2 shows a sub-method for recovering solvent from solvent-bearingmass. Step 1207 b includes maintaining at least a solvent-boiling pointtemperature for the extraction vessel and at least a solvent-condensingtemperature for a fluidly connected extraction system component. Forexample, solvent tank or other condensing component may be fluidlycoupled with an extraction vessel. Additionally or alternatively, afluidly connected extraction system component may be maintained at atemperature that is below the solvent-boiling point temperature, butabove the solvent-condensing temperature.

Step 1209 b includes monitoring a pressure of at least the extractionvessel and the fluidly connected extraction system component. Step 1212includes evaporating further residual solvent that remains in anextraction vessel if the monitored pressure indicates that residualsolvent remains in the solvent-bearing mass. In general, if residualsolvent remains within an extraction vessel, a vapor pressure (gauge)value may be an average of the vapor pressure of the heated extractionvessel and the cooled extraction system component (e.g., a cooledsolvent tank).

Upon the residual solvent being at least substantially removed from theextraction vessel, there is no further solvent to supply the vaporpressure. Thus, the measured pressure (whether it be measured at theextraction vessel, the fluidly coupled component, or a fluid linetherebetween) will drop and eventually matched the vapor pressure valueof the fluidly coupled component. For example, a cooled solvent tank ofbutane, at around 50° F./10° C. may have a vapor pressure of around 7psi_(g)/0.5 bar (by rounding up from the value shown in TABLE 1),indicating that a fluidly coupled extraction vessel, even if heated, isnot contributing to the vapor pressure average. Readings above around 7psi_(g)/0.5 bar would indicate a vapor-pressure contribution from theextraction vessel. That is, the vapor signature of residual butanesolvent remaining in an extraction vessel is generally above 7psi_(g)/0.5 bar in the case that a fluidly coupled extraction systemcomponent is containing solvent and held to around 50° F./10° C.

An assortment of example vapor pressure values for butane, propane, andmixtures thereof are shown in TABLE 1, below. In an example embodiment,said values of TABLE 1 or similar values may be stored in memory (e.g.,a look-up table) that is operably coupled to a controller for thecontroller to determine if residual solvent remains within an extractionvessel. In a further example embodiment, an operator (e.g., a user) ofthe extraction system can select which solvent or solvent blend. isbeing used or directly select the vapor pressure value. Based on theselected solvent or solvent blend (along with a measured orpredetermined vessel temperature value(s)), a controller can select oruse a particular vapor pressure value as a value that indicates thatresidual solvent emains in au extraction vessel. More generally, acontroller can determine if there is residual solvent remaining in theextraction vessel based on a selected vapor pressure value (e.g.,pre-selected by a user or a controller) or a determined vapor pressurevalue (e.g., a controller-calculated value based on vessel temperaturemeasurements) for a particular solvent or solvent blend.

TABLE 1 Vapor Pressure (psi_(g)/bar) Mixture Propane (C₃H₈) % 100 70 5030 0 Butane (C₄H₁₀) % 0 30 50 70 100 Temperature −44 0 0 0 0 0 (F./C.)−42.2 −30 6.8 0 0 0 0 −34.4 0.469 −20 11.5 4.7 0 0 0 −28.9 0.794 0.324−10 17.5 9 3.5 0 0 −23.3 1.21 0.621 0.242 0 24.5 15 7.6 2.3 0 −17.8 1.691.04 0.524 0.159 10 34 20.5 12.3 5.9 0 −12.2 2.35 1.41 0.849 0.407 20 4228 17.8 10.2 0 −6.67 2.9 1.93 1.23 0.704 30 53 36.5 24.5 15.4 0 −1.113.66 2.52 1.69 1.06 40 65 46 32.4 21.5 3.1 4.44 4.49 3.17 2.24 1.480.214 50 78 56 41 28.5 6.9 10 5.38 3.86 2.83 1.97 0.476 60 93 68 50 36.511.5 15.6 6.42 4.69 3.45 2.52 0.794 70 110 82 61 45 17 21.1 7.59 5.664.21 3.11 1.17 80 128 96 74 54 23 26.7 8.83 6.62 5.11 3.73 1.59 90 150114 88 66 30 32.2 10.4 7.87 6.07 4.55 2.07 100 177 134 104 79 38 37.812.2 9.25 7.18 5.45 2.62 110 204 158 122 93 47 43.3 14.1 10.9 8.42 6.423.24

FIG. 17 shows extraction system 1700, which omits the solute andsolute-solvent mixture lines for highlighting other aspects of system1700. Pressure sensors 618 a and 618 b are operably coupled,respectively, to extraction system component 617 and solvent tank 615 a.Controller 602 may be operably coupled to sensors 618 a and 618 b.Thermal element 612 may be heating vessel 611 while thermal element 111is cooling solvent tank 615 a. While vessel 611, component 617, and tank615 a are in fluid communication, the respective sensors 618, 618 a, and618 b should be providing an average vapor pressure, as explained above.

Alternatively or additionally, extraction system component 617 andvessel 611 may be isolated such that the extraction vessel 611 isotherwise sealed besides being fluid coupled to component 617. In suchembodiment, the pressure value from pressure sensor 618 a may reflectthe local vapor pressure of vessel 611, particularly when component 617is substantially devoid of, for example, condensed solvent and is of thesame or similar temperature of extraction vessel 611. Similarly,component 617 may isolate tank 615 a to determine the local vaporpressure of tank 615 a. In some cases, sensor 618 a may become moreaccurate in determining said local vapor pressure value when component617 is largely devoid of solvent vapor and is of the same or similartemperature as tank 615 a if, for example, tank 615 a is holdingcondensed solvent. In some embodiments, the above-described isolationmeasurements can be taken in addition to the above-described averagevapor pressure measurements.

FIG. 8 shows extraction system 1800, which omits the solute andsolute-solvent mixture lines for highlighting other aspects of system1800. Cold trap 620 may be maintained at a fluid-condensing temperaturethat condenses the heated fluid into a liquid fluid, but passes solventvapor, which condenses at a colder temperature in, for example, solventtank 615 a. For example, the heated fluid may be water vapor or steamand the solvent may be butane.

Cold trap 620 may be arranged directly above vessel 611 such that thecondensed liquid fluid may be gravity assisted in flowing back intovessel 611. Cold trap 620 may be in addition or an alternative tocooling vessel 611 to further ensure heated fluid does not reach tank615 a. Cold trap 620 may include a condenser and/or other vapor coolersfor condensing the heated fluid.

FIG. 19 shows extraction system 1900, which omits the solvent, solute,and solute-solvent mixture lines for highlighting other aspects ofsystem 1900. Vessel 611 may have a cross section that defines aplurality of channels 611 t that are physically separate from a centerchannel that contains a mass for extraction. Three possible crosssections are shown in FIGS. 8-7, 8-8, and 8-9, which show peripheralorifices 611 o that partially define said channels 611 t. In suchembodiments, heated (or cooled) fluid can be circulated through channels611 t and back to heated fluid source 610. Said circulation may be pumpassisted via optional pump 190. Channels 611 t are shown in a dashedline format to signify that channel 611 t is an internally defined spaceof vessel 611.

Additionally or alternatively, vessel 611 may be thermally regulated tocool said vessel 611. For example, a cooling fluid may be supplied tochannel 611 t for a cold extraction process or other thermal regulatingprocess such as condensing solvent or decreasing an extraction vesselpressure.

The disclosure above encompasses multiple distinct inventions withindependent utility. While each of these inventions has been disclosedin a particular form, the specific embodiments disclosed and illustratedabove are not to be considered in a limiting sense as numerousvariations are possible. For example, residual solvent can be removedfrom other extraction vessels that contain a solvent-bearing massbesides a vessel that is involved in (e.g., a first-pass) extraction ofa solute-bearing mass. For example, a solvent-hearing mass may bephysically removed from a first extraction vessel to a second extractionvessel such as a separator vessel, among other possible extractionsystem components, which otherwise performs the same residual-solventrecovery steps and methods. Such a separation vessel should also beunderstood as being an “extraction vessel” as it is removing residualsolvent from an extraction process while substantially maintaining thesolvent-bearing mass within said vessel. Additionally or alternatively,residual solvent may be removed from said mass before physically movingit out of the vessel that was also used for extracting solute from saidmass.

The subject matter of the inventions includes all novel and non-obviouscombinations and subcombinations of the various elements, features,functions and/or properties disclosed above and inherent to thoseskilled in the art pertaining to such inventions. Where the disclosureor subsequently filed claims recite “a” element, “a first” element, orany such equivalent term, the disclosure or claims should be understoodto incorporate one or more such elements, neither requiring norexcluding two or more such elements.

Applicant(s) reserves the right to submit claims directed tocombinations and subcombinations of the disclosed inventions that arebelieved to be novel and non-obvious. Inventions embodied in othercombinations and subcombinations of features, functions, elements and/orproperties may be claimed through amendment of those claims orpresentation of new claims in the present application or in a relatedapplication. Such amended or new claims, whether they are directed tothe same invention or a different invention and whether they aredifferent, broader, narrower or equal in scope to the original claims,are to be considered within the subject matter of the inventionsdescribed herein.

What is claimed is:
 1. A method of operating an extraction system forrecovering solvent from solvent-bearing mass, the method comprising:introducing, into an extraction vessel containing at least thesolvent-bearing mass, a first heated fluid portion into a first inputorifice of the extraction vessel, the first heated fluid portion havinga first temperature that is at least equal to a first solvent boilingpoint temperature; evaporating, by the first heated fluid portion, afirst liquid solvent portion from the solvent-bearing mass, therebyproducing a first solvent vapor portion; collecting at least the firstsolvent vapor portion after exiting a first output orifice of theextraction vessel; and at least substantially containing, during thecollecting the at least the first solvent vapor portion step, the firstheated fluid portion within the extraction vessel.
 2. The method ofclaim 1 with the solvent-bearing mass including solvent-bearing biomass.3. The method of claim 1 further comprising substantially maintainingthe first heated fluid portion at at least the first temperature as thefirst heated fluid portion travels through at least a portion of theextraction vessel that contains the solvent-bearing mass.
 4. The methodof claim 3 with the substantially maintaining step comprising heating,during the evaporating the first liquid solvent portion step, at leastone of the extraction vessel and an operably coupled extraction systemcomponent thereof for maintaining the first heated fluid portion at atleast the first temperature.
 5. The method of claim 1 with the at leastsubstantially containing step comprising closing at least the firstoutput orifice before the first heated fluid portion exits theextraction vessel.
 6. The method of claim 1 with the at leastsubstantially containing step comprising condensing the first heatedfluid portion and thereby producing a first liquid portion.
 7. Themethod of claim 6, with the condensing step comprising at least one ofincreasing a pressure within the extraction vessel, decreasing atemperature within the extraction vessel, and condensing the firstheated fluid portion by a cold trap that is arranged above theextraction vessel and downstream of the extraction vessel.
 8. The methodof claim 1 further comprising monitoring, by a controller, at least oneof a pressure and temperature of the extraction vessel.
 9. The method ofclaim 8 with the monitoring step comprising measuring at least oneextraction vessel temperature with at least one thermal sensor arrangedon or in the extraction vessel.
 10. The method of claim 8 with themonitoring step comprising monitoring a thermal gradient value across alength of the extraction vessel.
 11. The method of claim 8 with thefirst input orifice arranged on or near a first end portion of theextraction vessel and the first output orifice arranged on or near asecond end portion of the extraction vessel, the first and second endportion arranged on opposite ends of the extraction vessel, and with themonitoring step comprising monitoring, by the controller, at least atemperature of the second end portion of the extraction vessel.
 12. Themethod of claim 8 further comprising at least substantially stopping theintroduction step in response to a first monitored value that isobtained from the monitoring step, the first monitored value comprisingat least one of a first extraction vessel pressure value, a firstextraction vessel temperature value, and a first extraction vesselthermal gradient value.
 13. The method of claim 8 further comprisingclosing the extraction vessel in response to a second monitored valuethat is obtained from the monitoring step, the second monitored valuecomprising at least one of a second extraction vessel pressure value, asecond extraction vessel temperature value, and a second extractionvessel thermal gradient value.
 14. The method of claim 1 furthercomprising: monitoring a vapor pressure of the extraction vessel;determining if a monitored vapor pressure value indicates that residualsolvent remains in the extraction vessel, and if determined thatresidual solvent remains in the extraction vessel, the method furthercomprising: introducing a second heated fluid portion into the firstinput orifice or another input of the extraction vessel; substantiallymaintaining the second heated fluid portion in vapor form as the secondheated fluid portion travels through the extraction vessel; evaporating,by the first heated fluid portion, a second liquid solvent portion fromthe solvent-bearing mass, thereby producing a second solvent vaporportion; collecting at least the second solvent vapor portion afterexiting the first output orifice of the extraction vessel; and at leastsubstantially containing the second heated fluid portion within theextraction vessel.
 15. The method of claim 14, further comprisingsealing the extraction vessel or a fluidly coupled path thereof beforedetermining if the monitored vapor pressure value indicates thatresidual solvent remains in the extraction vessel.
 16. The method ofclaim 1 with the solvent-bearing mass comprising at least two solventswith differing boiling point temperatures, including the first solventboiling point temperature and a second solvent boiling pointtemperature, the method further comprising: introducing a second heatedfluid portion into the first input orifice or another input of theextraction vessel, the second heated portion being at a highertemperature than the first heated fluid portion and at least equal tothe second solvent boiling point; evaporating, by the second heatedfluid portion, a second liquid solvent portion from the solvent-bearingmass, thereby producing a second solvent vapor portion; collecting atleast the second solvent vapor portion after exiting the first outputorifice of the extraction vessel; and at least substantially containingthe second heated fluid portion within the extraction vessel.
 17. Themethod of claim 1 with the solvent-bearing mass comprising at least twosolvents with differing boiling point temperatures, including the firstsolvent boiling point temperature and a second solvent boiling pointtemperature that is higher than the first solvent boiling pointtemperature, the introducing the first heated fluid portion stepcomprising introducing, into the extraction vessel, the first heatedfluid portion into the first input orifice of the extraction vessel, thefirst heated fluid portion having the first temperature that is at leastequal to the second solvent boiling point temperature; and theevaporating step comprising evaporating, by the first heated fluidportion, the first liquid solvent portion from the solvent-bearing mass,thereby producing the first solvent vapor portion that comprises the atleast two solvents.
 18. The method of claim 1 with the introducing thefirst heated portion step comprising introducing, into the extractionvessel, a first heated vapor portion into the first input orifice of theextraction vessel.
 19. The method of claim 1, further comprisingevacuating, before introducing the first heated fluid portion, asolvent-solute mixture from the extraction vessel while retaining thesolvent-bearing mass within the extraction vessel.
 20. The method ofclaim 1, further comprising evacuating, after at least the evaporatingthe first liquid solvent portion step, at least one of the first heatedportion and a liquid portion thereof from the extraction vessel.
 21. Themethod of claim 1 with the first heated fluid portion comprising atleast one of a heated gas, heated CO₂, heated liquid water and watervapor.
 22. A method of thermally regulating an extraction vessel, themethod comprising: introducing, into the extraction vessel containing atleast a solvent-bearing mass, a first thermally regulated fluid portioninto a first plurality of input orifices of the extraction vessel, eachof the first plurality of input orifices partially defining anextraction vessel channel for transporting fluid along a length of theextraction vessel without the thermally regulated fluid contacting thesolvent-bearing mass; and thermally regulating, by the first thermallyregulated fluid portion, a first liquid solvent portion in contact withthe solvent-bearing mass.
 23. An extraction vessel comprising: anelongated vessel defining at least a first exterior shape and aninterior cavity; and a plurality of protrusions that (A) are arrangedwithin the elongated vessel, (B) extend into the cavity, and (C) arethermally coupled to the elongated vessel.
 24. The extraction vessel ofclaim 23 with the plurality of protrusions comprising a plurality offins that (A) are arranged within the elongated vessel, (B) extend intothe cavity, and (C) are thermally coupled to the elongated vessel. 25.The extraction vessel of claim 23 with each of the plurality ofprotrusions substantially spanning a length of the elongated vessels.26. The extraction vessel of claim 23 further comprising a thermaljacket that is thermally coupled to at least the plurality ofprotrusions.
 27. The extraction vessel of claim 26 with the thermaljacket mechanically coupled to an exterior portion of the elongatedvessel.
 28. The extraction vessel of claim 23 with the plurality ofprotrusions each comprising one or more heating elements.
 29. Theextraction vessel of claim 23 with the plurality of protrusions eachcomprising one or more resistive heating elements.
 30. The extractionvessel of claim 23 with the plurality of protrusions each defining acavity for transporting a heating fluid and/or cooling fluid across alength of the extraction vessel.
 31. The extraction vessel of claim 23with the plurality of protrusions each comprising a ferrous material.